Potassium Carbonate → 2-{[(6-Chloro(3-pyridyl))methyl][2-(2-ethylthio-3-nitropyrrolyl)ethyl]amino}ethanenitrile

HRID 549225노트

반응식

HRID 549225 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8]C(NCCCl)C#N)=[CH:4][CH:3]=1.[CH2:16]([S:18][C:19]1[NH:20][CH:21]=[CH:22][C:23]=1[N+:24]([O-:26])=[O:25])[CH3:17].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N:20]([CH2:21][CH2:22][C:22]2[C:23]([N+:24]([O-:26])=[O:25])=[C:19]([S:18][CH2:16][CH3:17])[NH:20][CH:21]=2)[CH2:19][C:23]#[N:24])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 598468692-Ethylthio-3-nitropyrroleHCID 86624866(6-Chloro(3-pyridyl)methyl] (2-chloroethylamino}ethanenitrile

생성물 1

HCID 866248682-{[(6-Chloro(3-pyridyl))methyl][2-(2-ethylthio-3-nitropyrrolyl)ethyl]amino}ethanenitrile

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

This compound was prepared in a manner analogous to that set forth in Step G of Example 1, using 0.17 gram (0.0007 mole) of 2-{[(6-chloro(3-pyridyl)methyl] (2-chloroethylamino}ethanenitrile (prepared in Steps A and B of the present Example), 0.10 gram (0.00064 mole) of 2-ethylthio-3-nitropyrrole and 0.22 gram (0.0016 mole) of potassium carbonate in about 15 mL of DMF. The crude product was purified with column chromatography on silica gel. Elution was accomplished using 50% hexane in diethyl ether and 100% diethyl ether as eluants. The appropriate fractions were combined and concentrated under reduced pressure, yielding 0.10 gram of Compound I. The NMR spectrum was consistent with the proposed structure.

후처리

  1. customThis compound was prepared in a manner analogous to that set forth in Step G of Example 1
  2. customThe crude product was purified with column chromatography on silica gel
  3. washElution
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ca0ddb384ff64c89a57728bcc045cb4e
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07943642B2

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